CN113038925A

CN113038925A - Oral composition

Info

Publication number: CN113038925A
Application number: CN201980075435.3A
Authority: CN
Inventors: 高桥康彦; 川延勇介
Original assignee: Lion Corp
Current assignee: Lion Corp
Priority date: 2018-12-26
Filing date: 2019-12-05
Publication date: 2021-06-25
Anticipated expiration: 2039-12-05
Also published as: JPWO2020137417A1; WO2020137417A1; CN113038925B; JP7363815B2; KR20210108938A

Abstract

The present invention provides an oral composition which has excellent retention in the oral cavity of tocopherol or a derivative thereof and has good appearance stability and usability. The oral composition contains (a) at least one selected from tocopherol and an ester thereof with an organic acid; (b) one or more selected from xanthan gum, alginate and carrageenan, and (c) polyacrylate with weight average molecular weight of 1,000-20,000.

Description

Oral composition

Technical Field

The present invention relates to an oral composition having excellent retention in the oral cavity of tocopherol or a derivative thereof and also having good appearance stability and usability.

Background

Since tocopherol or a derivative thereof has a peripheral circulation promoting effect (blood circulation promoting effect) in gingival tissues, it is useful for preventing periodontal diseases, and is widely blended in oral compositions such as dentifrice. In order to further improve the effects of these components, the improvement of retention in the oral cavity has been studied.

For example, patent document 1 (jp 2008-120753 a) proposes a technique of using hydroxyethyl cellulose as a non-anionic water-soluble polymer in order to improve the retention in the oral cavity of a vitamin E derivative, but the retention in the oral cavity is liable to be reduced by the influence of other components to be compounded, and there may be a problem in the stability of the preparation appearance and the like. On the other hand, patent document 2 (jp 2012-97057 a) proposes a technique of improving the persistence of foam during tooth brushing and the retention in the oral cavity of a medicinal ingredient such as vitamin E or a derivative thereof by using 1.4 mass% or more of xanthan gum and 1.4 mass% or more of alkyl sulfate in combination at a specific ratio and blending an amphoteric surfactant in combination, but the amount of xanthan gum is relatively large, and therefore the extrusion from a tube container is not easy under low-temperature storage conditions and the usability is deteriorated in some cases.

Documents of the prior art

Patent document

Patent document 1: japanese patent laid-open No. 2008-120753

Patent document 2: japanese laid-open patent publication No. 2012-97057

Disclosure of Invention

Problems to be solved by the invention

The present invention has been made in view of the above circumstances, and an object thereof is to provide an oral composition having excellent retention in the oral cavity of tocopherol or a derivative thereof, and also having good appearance stability and usability.

Technical scheme for solving problems

The present inventors have conducted extensive studies to achieve the above object and found that: when a polyacrylate salt having a weight average molecular weight of a specific value or less is used in combination with a water-soluble polymer substance in an oral composition containing a specific tocopherol or a derivative thereof, a remarkable oral retention effect of the tocopherol or the derivative thereof is exhibited, the oral retention is excellent, and appearance stability and usability can be maintained well. Namely, it was found that: in the present invention, an oral composition having excellent retention in the oral cavity of component (a), suppressed liquid separation even after storage at high temperature, good appearance stability, easy extrusion from a storage container even after storage at low temperature, and good usability can be obtained by compounding (a) at least one member selected from the group consisting of tocopherol and esters thereof with organic acids, (b) at least one member selected from the group consisting of xanthan gum, alginate, and carrageenan (carrageenan), and (c) a polyacrylate having a weight average molecular weight of 1,000 to 20,000, and the present invention has been completed.

As the binder for an oral composition, polyacrylic acid or a salt thereof is known, and a crosslinked polyacrylic acid or a salt thereof having a weight average molecular weight of 10 ten thousand or more, usually about 30 ten thousand is generally used. On the other hand, in the present invention, it is clarified that the use of (c) a polyacrylate salt having a low weight average molecular weight of 20,000 or less (preferably a linear polyacrylate salt) in combination with the component (b) serves to improve the retention in the oral cavity of the component (a), whereby excellent retention in the oral cavity can be imparted while maintaining good appearance stability and usability as described above. Therefore, by combining the components (a), (b) and (c), the retention in the oral cavity of the component (a) can be improved and made excellent without increasing the amount of the water-soluble polymer such as xanthan gum, and the above-mentioned remarkably advantageous effects can be imparted. The relevant effect cannot be achieved in the following cases: instead of using the component (c), a polyacrylate salt having a weight average molecular weight of more than 20,000 or polyacrylic acid having a weight average molecular weight of 20,000 or less but not in the form of a salt is used.

It is clear from the results of comparative examples described later that when component (c) is not contained, component (a) is inferior in retention in the oral cavity even when component (b) is contained and polyacrylate having a weight average molecular weight of 300,000 is contained (comparative examples 1 and 3). In this case, comparative example 1 containing no polyacrylate was also inferior in appearance stability (presence or absence of liquid separation) after high-temperature storage, and comparative example 3 containing a polyacrylate having a weight average molecular weight of 300,000 was also inferior in ease of extrusion from the container after low-temperature storage. When the component (b) is not contained, even if the component (c) is contained, the retention in the oral cavity of the component (a) is poor and the appearance stability (presence or absence of liquid separation) after storage at high temperature is also poor (comparative example 2).

Further, when component (c) is not contained, even when component (b) and polyacrylic acid having a weight average molecular weight of 20,000 or less are contained, component (a) has poor retention in the oral cavity.

On the other hand, in the oral composition of the present invention containing the components (a), (b) and (c) shown in the examples, the component (a) is retained in the oral cavity at a high rate, and the retention in the oral cavity of the component (a) is excellent, and further, the appearance stability (presence or absence of liquid separation) after storage at high temperature and the ease of extrusion from the container after storage at low temperature are also excellent.

In patent document 2, the oral retention of vitamin E or a derivative thereof is improved by a combination of xanthan gum, an alkyl sulfate and an amphoteric surfactant, whereas in the present invention, the oral retention of component (a) is improved by components (b) and (c), and the appearance stability and the usability after low-temperature storage can be ensured.

Accordingly, the present invention provides the following oral compositions:

[ 1] an oral composition comprising:

(a) one or more selected from tocopherol and esters thereof with organic acids;

(b) one or more selected from xanthan gum (xanthan gum), alginate and carrageenan; and the number of the first and second groups,

(c) a polyacrylate salt having a weight average molecular weight of 1,000 or more and 20,000 or less.

[ 2] the oral composition according to [ 1], wherein the component (a) is selected from the group consisting of tocopherol, tocopherol acetate and tocopherol nicotinate.

[ 3] the oral composition according to [ 1] or [ 2], wherein the polyacrylate salt has a weight average molecular weight of 5,000 to 10,000.

[ 4 ] the oral composition according to any one of [ 1] to [ 3], wherein the mass ratio of (c)/(b) is 0.1 to 3.

The oral composition according to any one of [ 1] to [ 4 ], wherein ((b) + (c))/(a) is 1 to 30 in mass ratio.

The oral composition according to any one of [ 1] to [ 5 ], wherein the content of the component (b) is 0.4 to 1.4% by mass, and the content of the component (c) is 0.1 to 2% by mass.

The oral composition according to any one of [ 1] to [ 6 ], wherein the content of the component (a) is 0.05 to 1% by mass.

The oral composition according to any one of [ 1] to [ 7 ], wherein the oral composition is a dentifrice composition.

Effects of the invention

According to the present invention, it is possible to provide an oral composition which has excellent retention in the oral cavity of the component (a) and has good appearance stability and usability. The oral composition of the present invention can sufficiently exhibit the drug effect of the component (a), and is effective for preventing or inhibiting periodontal diseases such as gingivitis and periodontitis.

Detailed Description

The present invention will be described in more detail below. The oral composition of the present invention comprises: (a) one or more selected from tocopherol and esters thereof with organic acids; (b) one or more selected from xanthan gum, alginate and carrageenan; and (c) a polyacrylate having a weight average molecular weight of 1,000 to 20,000.

(a) The component (C) is tocopherol or a derivative of tocopherol, and an ester of tocopherol and an organic acid can be used as the derivative of tocopherol. These may be used alone or in combination of two or more selected from these. (a) The component (A) is a medicinal component having the effects of promoting blood flow and repairing tissue, and is effective in preventing or inhibiting periodontal diseases such as gingivitis and periodontitis.

Examples of the tocopherol include: d-alpha-tocopherol, dl-alpha-tocopherol, beta-tocopherol, gamma-tocopherol, delta-tocopherol, and the like.

The ester of tocopherol with an organic acid may be an ester of tocopherol with an organic acid such as acetic acid, nicotinic acid, succinic acid, linolenic acid, or a salt thereof. Specific examples thereof include: tocopheryl acetates such as d- α -tocopheryl acetate and dl- α -tocopheryl acetate; tocopherol nicotinates such as d- α -tocopherol nicotinate and dl- α -tocopherol nicotinate; tocopherol succinates such as d- α -tocopherol succinate and dl- α -tocopherol succinate; tocopherol linolenates such as d-alpha-tocopherol linolenate and dl-alpha-tocopherol linolenate; calcium tocopheryl succinate. Among them, from the viewpoint of retention in the oral cavity, tocopherol acetate and tocopherol nicotinate are preferable, and tocopherol acetate is particularly preferable.

(a) The components can be used in compliance with the standards of used cosmetic materials in Japan (cosmetic bases) or the standards 2006 for raw materials for foreign products in Japan pharmaceutical department, and commercially available products such as those manufactured by DSM Nutrition Japan K.K., sanitary food chemical Co., Ltd., BASF Japan, etc. can be used.

The amount of the component (a) is preferably 0.05 to 1% by mass of the entire composition, more preferably 0.08 to 1.0%, and still more preferably 0.1 to 0.5%, from the viewpoint of the effectiveness and taste. When the amount of the component is within the above range, the retention in the oral cavity is sufficiently improved, and the component is sufficiently soluble in the composition, so that the appearance stability and the taste are also excellent even after storage at high temperature.

(b) The component is one or more selected from xanthan gum, alginate and carrageenan. These are anionic water-soluble polymer substances, and contribute to improvement of retention in the oral cavity of component (a).

The alginate may be an alkali metal salt such as sodium alginate, and is preferably sodium alginate.

From the viewpoint of intraoral retention of component (a), component (b) is particularly preferably xanthan gum or carrageenan, and more preferably xanthan gum.

(b) As the component (C), commercially available products such as those manufactured by CP Kelco, KIMICA, Tribuli, etc. can be used.

(b) The amount of the component (B) is preferably 0.4 to 1.4%, more preferably 0.6 to 1.0% of the total composition. When the blending amount is 0.4% or more, the retention in the oral cavity of the component (a) is very excellent, and the appearance stability after storage at high temperature can be sufficiently obtained. When the mixing amount is 1.4% or less, the ease of extrusion from the container after storage at low temperature can be sufficiently maintained.

(c) The component (B) is a polyacrylate having a weight average molecular weight (Mw) of 1,000 to 20,000. (c) The component (a) acts to improve retention in the oral cavity, and also contributes to suppression of liquid separation after storage at high temperature and securing of easiness of extrusion from a container after storage at low temperature.

The weight average molecular weight of the polyacrylate salt of component (c) is 1,000 or more, preferably 5,000 or more, particularly 6,000 or more, and further 20,000 or less, preferably 10,000 or less, particularly 8,000 or less, from the viewpoint of retention in the oral cavity and appearance stability of component (a). When the weight average molecular weight is less than 1,000, the effect of improving the retention in the oral cavity of the component (a) is poor, and the appearance stability after storage at high temperature is poor. When the weight average molecular weight is more than 20,000, the effect of improving the intraoral retention of component (a) is reduced, and the intraoral retention of component (a) cannot be sufficiently obtained.

The polyacrylate salt of the component (c) has a weight average molecular weight of preferably 5,000 to 20,000, more preferably 5,000 to 10,000, from the viewpoint of retention in the oral cavity of the component (a).

The weight average molecular weight is measured by GPC (gel permeation chromatography) according to the method and measurement conditions described in japanese patent No. 5740859. The details are as follows (the same applies below).

Method for measuring weight average molecular weight:

the weight average molecular weight is a value measured using a gel permeation chromatograph/multi-angle laser light scattering detector (GPC-MALLS), and the conditions are as follows.

Mobile phase: 0.3M NaClO₄

NaN₃Aqueous solution column: TSKgel alpha-M2 root

Pre-column (precolumn): TSKguardcolumn alpha

Standard substance: polyethylene glycol

The polyacrylate salt of the component (c) is preferably a linear polyacrylate salt (non-crosslinked polyacrylate salt) from the viewpoint of intraoral retention of the component (a).

The salt is preferably a monovalent salt, more preferably an alkali metal salt or an ammonium salt, still more preferably an alkali metal salt such as a sodium salt or a potassium salt, and particularly preferably a sodium salt.

As such a polyacrylate, commercially available products sold by Polyscience corporation or Toyo Synthesis Co., Ltd can be used.

As specific commercially available products, sodium polyacrylate (Mw: 1,000); straight-chain, sodium polyacrylate (Mw: 6,000) manufactured by Polyscience; straight-chain, available from Toyo Synthesis Co., Ltd., AC-10NP, AC-10NPD, ARON T-50, sodium polyacrylate (Mw: 8,000); straight-chain, sodium polyacrylate (Mw: 20,000) manufactured by Polyscience; linear, ARON A-20UN manufactured by Toyo Synthesis K.K..

The polyacrylate salt of component (c) has a weight average molecular weight lower than that of a crosslinked polyacrylate salt of a binder used in a usual dentifrice and is different from a polyacrylate salt known as a binder.

(c) The amount of the component (b) is preferably 0.1 to 2%, more preferably 0.3 to 1.0%, and further preferably 0.4 to 0.8% of the total composition. When the blending amount is 0.1% or more, the retention in the oral cavity of the component (a) is sufficiently improved, and the appearance stability after storage at high temperature can be sufficiently obtained. When the blending amount is 2% or less, the influence of the taste of the component (c) itself can be sufficiently prevented.

Further, in the present invention, (c)/(b) which represents the amount ratio of the component (b) to the component (c) is preferably 0.1 to 3, more preferably 0.3 to 1.5, and further preferably 0.5 to 1.0 in terms of mass ratio. When the mass ratio of (c)/(b) is within the above range, the component (a) is more excellent in retention in the oral cavity, and also excellent in appearance stability (presence or absence of liquid separation) after high-temperature storage and easiness of extrusion from a container after low-temperature storage.

Further, the mass ratio of ((b) + (c))/(a) representing the amount ratio of the component (a) to the components (b) and (c) is preferably 1 to 30, more preferably 1 to 20, and still more preferably 1 to 16. When the mass ratio of ((b) + (c))/(a) is within the above range, the component (a) is more excellent in retention in the oral cavity, and is more excellent in appearance stability (presence or absence of liquid separation) after high-temperature storage and ease of extrusion from a container after low-temperature storage.

In the present invention, particularly, when the mass ratio of (c)/(b) to ((b) + (c))/(a) is within the above range, the retention in the oral cavity of the component (a) is further improved, and the appearance stability (presence or absence of liquid separation) after high-temperature storage and the ease of extrusion from the container after low-temperature storage are further improved, which is particularly preferable.

The oral composition of the present invention can be formulated into a dentifrice in a paste, gel or liquid form (e.g., a paste dentifrice, a gel dentifrice, a liquid dentifrice, etc.), a mouth rinse, an oral spray, a coating agent, a patch, etc., and is particularly suitable as a dentifrice composition (particularly, a paste dentifrice composition). In this case, as optional components in addition to the above components, known components other than the above may be blended as necessary depending on the dosage form and the like. The optional ingredients are preferably added within a range not affecting the effect of the present invention. Specifically, a dentifrice composition such as a dentifrice in the form of a paste may be blended with an abrasive, a binder, a thickener, a surfactant, a sweetener, a preservative, a coloring agent, a perfume, an active ingredient, and the like, and these ingredients may be mixed with water and prepared by a usual method. The blending amount shown below is an amount based on the entire composition.

Examples of the polishing agent include: silica-based abrasives such as silicic anhydride, crystalline silica, amorphous silica, silica gel, and aluminosilicate; calcium phosphate-based abrasives such as tricalcium phosphate, tetracalcium phosphate, anhydrous calcium hydrogen phosphate, and calcium hydrogen phosphate dihydrate; zeolite, calcium pyrophosphate, calcium carbonate, sodium bicarbonate, aluminum hydroxide, alumina, magnesium carbonate, trimagnesium phosphate, zirconium silicate, hydroxyapatite, and synthetic resin-based abrasive. These may be used singly or in combination of two or more, and among them, from the viewpoint of usability, a silica-based polishing agent such as silicic anhydride or a calcium phosphate-based polishing agent is preferable as the inorganic polishing agent, and silicic anhydride is particularly preferable (the compounding amount is usually 5 to 60%, and 10 to 55% in the case of a dentifrice in the form of a paste).

Examples of the binder include: an organic binder other than the component (b), or an inorganic binder such as silica gel, aluminum silica gel (aluminum silica gel), magnesium aluminum silicate (Veegum), or synthetic layered silicate (Laponite) (the compounding amount is usually 0.3 to 10%, and the compounding amount of the inorganic binder may be 1 to 5%).

In the present invention, since the component (b) can also function as a binder, an organic binder other than the component (b) may not be added (mixing amount is 0%).

Examples of the thickener include: sugar alcohols such as sorbitol, maltitol, lactitol and erythritol, and polyhydric alcohols such as propylene glycol (the blending amount is usually 5 to 70%).

The surfactant may be mixed with an anionic surfactant, a nonionic surfactant, or an amphoteric surfactant. These may be used singly or in combination.

Examples of the anionic surfactant include: alkyl sulfates, acyl amino acid salts, acyl taurates, and the like having an alkyl group having 12 to 14 carbon atoms. The acyl group of the acylamino acid salt and the acyl taurate has 12 to 14 carbon atoms, and particularly 12 carbon atoms.

Specifically, examples of the alkyl sulfate include: lauryl sulfate, myristyl sulfate; examples of the acylamino acid salt include: acyl glutamates such as lauroyl glutamate and myristoyl glutamate, and acyl sarcosinates such as lauroyl sarcosinate; examples of acyl taurates include: lauroyl methyl taurate. The salt is preferably an alkali metal salt such as sodium salt or potassium salt. Particularly preferred are alkyl sulfates, acyl sarcosinates, and acyl taurates. Among these, anionic surfactants having a hydrocarbon group (lauryl group) having 12 carbon atoms are preferable, and particularly, alkyl sulfate (sodium salt) is more preferable because it has a better taste than other surfactants.

Examples of the nonionic surfactant include: polyoxyethylene alkyl ether, polyoxyethylene-polyoxypropylene block copolymer, polyoxyethylene hydrogenated castor oil, polyoxyethylene ether of glyceride, sucrose fatty acid ester, alkanolamide, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, and fatty acid glyceride. Among them, polyoxyethylene alkyl ethers, polyoxyethylene hydrogenated castor oils, alkanolamides, and sorbitan fatty acid esters are preferable from the viewpoint of general versatility. The polyoxyethylene alkyl ether has an alkyl chain having 14 to 30 carbon atoms and preferably has an average number of moles of ethylene oxide added (average number of EO added) of 3 to 30. The average addition EO of the polyoxyethylene hydrogenated castor oil is preferably 5 to 100, and more preferably 20 to 60. The number of carbon atoms in the alkyl chain of the alkanolamide is preferably 12 to 14. The number of carbon atoms of the fatty acid in the sorbitan fatty acid ester is preferably 12 to 18. In the polyoxyethylene sorbitan fatty acid ester, the number of carbon atoms of the fatty acid is preferably 16 to 18, and the average addition EO is preferably 10 to 40.

Examples of the amphoteric surfactant include: acylamino acetic acid betaine and fatty acid amide propyl betaine having an acyl group with 12 to 14 carbon atoms. Examples of the acylaminoacetic acid betaine include: lauroyl dimethyl aminoacetic acid betaine, examples of fatty acid amide propyl betaine include: coco fatty acid amide propyl betaine.

The amount of the surfactant to be blended is usually 0.01 to 15%, particularly 0.01 to 10%.

The amount of the anionic surfactant may be 0.1 to 3%, particularly 0.5 to 2%. The amount of the alkyl sulfate may be 1.2% or less, particularly 1.0% or less, and further 0.8% or less. The mixing amount of the nonionic surfactant is preferably 0.01 to 10%. The blending amount of the amphoteric surfactant is preferably 0 to 3%.

Examples of the sweetener include: saccharin sodium, stevioside, dipotassium glycyrrhizinate, perillaseed, thaumatin (thaumatin), neohesperidin dihydrochalcone and aspartyl phenylalanine methyl ester.

Examples of the preservative include: parabens and sodium benzoate.

The colorant includes: blue No. 1, yellow No. 4, titanium dioxide.

As the flavor, known flavor materials used in the following oral compositions can be used: such as peppermint oil (peppermint oil), spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cinnamon oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, citrus oil (mandarin oil), lime oil (lime oil), lavender oil, rosemary oil, bay oil, chamomile oil (chamomile oil), caraway oil, marjoram oil (marjoram oil), bay leaf oil, lemongrass oil, oregano oil, pine needle oil, orange oil (neroli oil), rose oil, jasmine oil, iris extract, peppermint oil, rose oil, neroli oil, and the like, and these natural fragrances are processed (prefractionation, defecate fraction, fractionation, liquid-liquid extraction, refinement, powder fragrance, etc.), and menthol, carvone, menthyl salicylate, 3-1-propane, 2-diol, linalool, linalyl acetate, limonene, menthone, menthyl acetate, N-substituted-p-menthane-3-carboxamide, pinene, octanal, citral, pulegone, carvyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexylpropionate, methyl anthranilate, ethyl methylphenylglycidylate, vanillin, undecalactone, hexanal, isoamyl alcohol, hexenol, dimethyl sulfide, methylcyclopentenone (cyclotene), furfural, trimethylpyrazine, ethyl lactate, ethyl thioglycolate and other simple perfumes, further, blending flavors such as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, cream flavor, milk flavor, mixed fruit flavor, tropical fruit flavor, and the like are not limited to the flavors of the examples.

The perfume raw material is preferably used in an amount of 0.000001 to 1% of the total composition. As the perfuming agent using the perfume raw material, 0.001-2.0% of the composition is preferably used.

Examples of the optional active ingredients include: nonionic bactericides such as isopropyl methylphenol; cationic bactericides such as cetylpyridinium chloride (cetylpyridinium chloride); enzymes such as dextranase, mutanase, lysozyme, amylase, protease, lysozyme, and SOD (superoxide dismutase); alkali metal monofluorophosphates such as sodium monofluorophosphate and potassium monofluorophosphate; fluorides such as sodium fluoride and stannous fluoride; anti-inflammatory agents such as tranexamic acid, epsilon-aminocaproic acid, allantoin chlorohydroxyaluminum, dihydrocholesterol, glycyrrhizic acid, glycyrrhetinic acid, etc.; hypersensitive improvers such as potassium nitrate and aluminum lactate; a glycerophosphate salt; chlorophyll; sodium chloride; zinc compounds such as zinc chloride, zinc oxide, and zinc citrate; copper compounds such as copper gluconate and copper sulfate; vitamins such as vitamin a, vitamin B group, vitamin C, and the like; cortex Phellodendri and folium Camelliae sinensis. These active ingredients may be used alone or in combination in an effective amount within a range not to impair the effects of the present invention.

The pH (25 ℃) of the oral composition may be in the usual range, and is preferably 5 to 9, particularly preferably 6 to 8. The pH can be adjusted by adding a known pH adjuster, for example, a hydroxide of an alkali metal such as hydrochloric acid or sodium hydroxide.

Examples

The present invention will be specifically described below by way of examples and comparative examples, but the present invention is not limited to the following examples. In the following examples,% represents% by mass unless otherwise specified.

[ examples and comparative examples ]

Dentifrice compositions (dentifrice in paste form) having the compositions shown in tables 1 to 3 were prepared by a conventional method and evaluated by the following method, and the results are also shown in tables 1 to 3.

(1) Method for evaluating intraoral retention of tocopherol or derivative thereof

The skin of a 7-week-old male hairless rat (Labskin, Japan SLC Corp.) cut to 1.5cm square was placed on a 6-well plate, and 5mL of artificial saliva (50mM KCl, 1mM CaCl) was added₂，0.1mM MgCl₂，1mM KH₂PO₄Ph7.0), and left standing for 2 hours. A glass frame was placed on the skin so as to have a transmission area (about 0.8 cm)²) At a constant volume, 300. mu.L of each dentifrice composition of each example, 5g of which was diluted 3-fold with artificial saliva, was poured and allowed to stand for 5 minutes. Then, the dilution was discarded, 5mL of water was added, and the mixture was washed at 160rpm for 1 minute using a shaker. The above washing was repeated for 2 times in total.

The washing solution was discarded, and the skin was collected in a tube, and 1mL of ethanol (EtOH 90%) was added thereto, followed by extraction with a vortex mixer for 5 minutes. The extract was recovered, diluted with methanol in an equal fold, and then tocopherol or a derivative thereof (component (a)) was quantified by an absolute calibration curve method by HPLC (high performance liquid chromatography using the following instrument) under the following test conditions.

Instrument for use

The pump: LC-20AD, Shimadzu corporation

The sample introduction section: SIL-20AC, Shimadzu Kaisha Shimadzu

The detector: shimadzu corporation, SPD-20A

Column thermostat: CTO-20AC, Shimadzu corporation

Eluent flow rate: 1mL/min

Test conditions

The detector: ultraviolet absorption photometer (measuring wavelength: 273nm)

Column: COSMOSIL 5C₁₈-MS-II

Column temperature: 40 deg.C

Eluent: methanol

As a control, the intraoral retention rate (%) of the component (a) when treated with each dentifrice composition was calculated, taking the quantitative value of tocopherol or a derivative thereof when treated with the dentifrice composition of comparative example 1 as 100%. Among these, with respect to the control products of examples 16 and 17, the component (a) of comparative example 1 was changed to tocopherol nicotinate (the same substance as in example 16) and tocopherol (the same substance as in example 17). Further, with respect to the control products of examples 18 and 19, the tocopherol acetate amount of comparative example 1 was changed to 0.5% (the same amount as in example 18) and 1.0% (the same amount as in example 19), respectively.

In the oral retention of tocopherol or a derivative thereof (component (a)), the oral retention rate of 110% or more was judged as excellent and acceptable, the oral retention rate of 120% or more was judged as more excellent, the oral retention rate of 130% or more was judged as more excellent, and the oral retention rate of 140% or more was judged as the most excellent.

(2) Method for evaluating appearance stability (presence or absence of liquid separation) after high-temperature storage

A dentifrice composition (50 g) was filled in a laminated tube container having an aperture of 8mm, and 3 tubes of each composition were stored at 50 ℃ for 1 month. After leaving at room temperature, 10cm of the dentifrice composition was extruded from the above tube container onto a straw paper, and when the liquid separation was observed at the edge of the mouth of the container and the liquid exuded from the straw paper, the length of the liquid was measured, and the degree of liquid separation was evaluated based on the following scale.

The average of the evaluation scores of 3 tubes was calculated, and the appearance stability (presence or absence of liquid separation) after high-temperature storage was determined based on the following evaluation criteria.

Grading standard:

and 4, dividing: no liquid separation is observed at all during extrusion;

and 3, dividing: during extrusion, basically no liquid separation (less than 1cm) exists, and no problem exists in use;

and 2, dividing: during extrusion, liquid separation of 1-2 cm is found at the edge part of the opening;

1 minute: upon extrusion, the edge portion of the mouth was found to have more than 2cm of liquid separation.

Evaluation criteria:

very good: 3.5 minutes or more and 4.0 minutes or less;

o: 3.0 minutes or more and less than 3.5 minutes;

and (delta): 2.0 min or more and less than 3.0 min;

x: less than 2.0 minutes.

(3) Method for evaluating ease of extrusion from container after low-temperature storage

A dentifrice composition (50 g) was filled in a laminated tube container having an aperture of 8mm, and each of 3 tubes of each composition was stored at-5 ℃ for 1 month. After standing to room temperature, the dentifrice composition was extruded from the above tube container, and the ease of extrusion from the container was evaluated according to the rating scale described below.

The average of the evaluation scores of 3 tubes was calculated, and the ease of extrusion from the container after low-temperature storage was determined based on the evaluation criteria described below.

Grading standard:

4, dividing; can be smoothly extruded from the tube container;

3 min; can be extruded from the tube container somewhat smoothly;

2 min; slightly harder to extrude from a tube container;

1 minute; difficult to extrude from a tube container.

Evaluation criteria:

very good: 3.5 minutes or more and 4.0 minutes or less;

o: 3.0 minutes or more and less than 3.5 minutes;

and (delta): 2.0 min or more and less than 3.0 min;

x: less than 2.0 minutes.

Details of the raw materials used are as follows:

(a) composition (I)

Tocopherol acetate

dl-alpha-tocopheryl acetate, manufactured by DSM Nutrition Japan K.K

Tocopheryl nicotinate

Vitamin E nicotinate manufactured by BASF Japan K.K

Tocopherol

dl-alpha-tocopherol, manufactured by BASF Japan K.K

(b) Composition (I)

Xanthan gum

Manufactured by Monat Gum DA, CP Kelco

Sodium alginate

KIMILOID, KIMICA, Inc

Carrageenan

GENUVISCO (registered trademark) J-J, manufactured by TRICRYSTALLINE CORPORATION

(c) Composition (I)

Sodium polyacrylate (Mw: 1,000)

Straight-chain sodium polyacrylate (Mw: 1,000) manufactured by Polysciences

Sodium polyacrylate (Mw: 6,000)

Straight-chain Jurymer AC-10NP manufactured by Toyo chemical Co., Ltd

Sodium polyacrylate (Mw: 8,000)

Straight-chain sodium polyacrylate (Mw: 8,000) manufactured by Polysciences

Sodium polyacrylate (Mw: 20,000)

Straight-chain, ARON A-20UN, manufactured by TOYA SYNTHETIC CO., LTD

Sodium polyacrylate (Mw: 300,000) (comparison product)

Crosslinked type, sodium polyacrylate (Mw: 300,000), manufactured by Polysciences

[ Table 1]

[ Table 2]

[ Table 3]

Claims

1. An oral composition comprising:

(a) one or more selected from tocopherol and esters thereof with organic acids;

(b) one or more selected from xanthan gum, alginate and carrageenan; and the number of the first and second groups,

2. The oral composition according to claim 1, wherein the component (a) is selected from the group consisting of tocopherol, tocopherol acetate, and tocopherol nicotinate.

3. The oral composition according to claim 1 or 2, wherein the polyacrylate salt has a weight average molecular weight of 5,000 or more and 10,000 or less.

4. The oral composition according to any one of claims 1 to 3, wherein the mass ratio of (c)/(b) is 0.1 to 3.

5. The oral composition according to any one of claims 1 to 4, wherein ((b) + (c))/(a) is 1 to 30 in mass ratio.

6. The oral composition according to any one of claims 1 to 5, wherein the content of the component (b) is 0.4 to 1.4% by mass and the content of the component (c) is 0.1 to 2% by mass.

7. The oral composition according to any one of claims 1 to 6, wherein the content of the component (a) is 0.05 to 1% by mass.

8. The oral composition according to any one of claims 1 to 7 wherein the oral composition is a dentifrice composition.